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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 653-656 
    ISSN: 0009-2940
    Keywords: Hydroxylamine, O-methyl-N,N-bis(trifluoromethyl)-, gas-phase structure of ; Electron diffraction ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The molecular structure of (CF3)2NOCH3 was determined by gas electron diffraction. The molecular intensities were reproduced by use of a single conformation with syn orientation of the O-CH3 group relative to the nitrogen lone pair. This was confirmed by ab initio calculations (HF/3-21G(*), polarization functions only on nitrogen, and MP2/6-31G*). The observed structure demonstrates that the generalized anomeric effect is of minor importance to this compound. The following skeletal geometric parameters (bond lengths [pm] and angles [°] with 3-s̰ uncertainties) were derived: N-C 142.9(7), N-O 142(3), O-C 145(3), CNC 118.0(9), CNO 108.1(17), and NOC 109.4(17). The experimental structure is well reproduced by the ab initio calculations.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1749-1755 
    ISSN: 0044-2313
    Keywords: Tetramethylammonium trifluormethoxytrifluormethyliodate(I) ; Tetramethylammonium fluorotrifluormethyliodate(I) ; Tetramethylammonium chlorotrifluormethyliodate(I) ; Tetramethylammonium bromotrifluormethyliodate(I) ; vibrational spectra ; 19F13C NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Trifluormethylhalogen Iodate(I) Salts (CH3)4N+CF3IX- (X = F, Cl, Br) and Trifluormethyltrifluormethoxy Iodate(I) (CH3)4N+CF3IOCF3-We describe the preparation of new trifluormethyliodate(I) salts CF3IX- (X = F, Cl, Br, OCF3). (CH3)4N+CF3ICl- and (CH3)4N+CF3IBr- are obtained via addition of CF3I with the corresponded tetramethylammonium halogenide. (CH3)4N+CF3IOCF3- is synthesized by comproportionation of (CH3)4N+CF3ICl- with CF3OCl under formation of Cl2 at -78°C. (CH3)4N+CF3IF- is formed either, through thermolysis of (CH3)4N+ CF3IOCF3- under separation of COF2, or reaction of CF3I with (CH3)4N+ OCF3-. The thermolabile compounds have been characterized by i.r., Raman, 19F-, 13C NMR spectroscopy.
    Notes: Es wird über die Darstellung einer Reihe neuer Iodate(I) des Typs CF3IX- (X = F, Cl, Br, OCF3) berichtet. (CH3)4N+CF3ICl- und (CH3)4N+CF3IBr- werden durch Additionsreaktion von CF3I an die entsprechenden Tetramethylammoniumhalogenide dargestellt. (CH3)4N+CF3IOCF3- erhält man durch Komproportionierung von (CH3)4N+CF3ICl- mit CF3OCl bei -78°C. CF3IF- entsteht sowohl, durch die Thermolyse von (CH3)4N+ CF3IOCF3- unter Abspaltung von COF2 bei -20°C, als auch durch Umsetzung von CF3I mit (CH3)4N+OCF3- bei -20°C.Die thermolabilen Verbindungen werden durch IR-, Raman-sowie Multikern-NMR-Spektroskopie charakterisiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1404-1410 
    ISSN: 0044-2313
    Keywords: Dihydroxycarbeniumion ; crystal structure ; vibrational spectra ; NMR-spectra ; superacid reaction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dihydroxycarbeniumhexafluorometallates - Synthesis, Spectroscopic Characterization, and Crystal Structure of HC(OH)2+AsF6-The preparation of HC(OH)2+ MF6- (M = As, Sb) by protonation of HCOOH in the superacid systems HF/MF5 is reported. The very hydrolysable and thermolabile salts are characterized by vibrational and NMR spectroscopic methods. Under inert conditions they are stable at -40°C for some weeks. HC(OH)2+AsF6- crystallizes in the orthorhombic space group Pbca (No. 61) with a = 965.8(1), b = 1582.20(16), c = 766.40(8) pm with eight formula units per unit cell.
    Notes: Es wird über die Darstellung von HC(OH)2+MF6- (M = As, Sb) durch Protonierung von Ameisensäure in den supersauren Systemen HF/MF5 berichtet. Die hydrolyseempfindlichen und thermolabilen Dihydroxycarbeniumsalze werden schwingungs- und NMR-spektroskopisch charakterisiert. Sie sind unter inerten Bedingungen bei -40°C wochenlang haltbar.HC(OH)2+AsF6- kristallisiert in der orthorhombischen Raumgruppe Pbca (Nr. 61) mit den Gitterkonstanten a = 965,8(1), b = 1582,20(16) und c = 766,40(8) pm mit acht Formeleinheiten in der Elementarzelle.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 557-561 
    ISSN: 0044-2313
    Keywords: Thiosulfonium salts ; preparation ; vibrational, NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Preparation of Di(i-propyl)thiosulfonium Salts [1]The preparation of the mercaptosulfonium salts (i-C3H7)2SSX+SbCl6- (X = H, D) and of the chlorothiosulfonium salts (i-C3H7)2SSCl+MF6- (M = As, Sb) and (i-C3H7)2SSSCl+SbCl6- is reported. They are formed by reaction of chlorinated or protonated (i-C3H7)2S with excess H2S or SCl2 and S2Cl2. The thiosulfonium compounds are characterized by vibrational and NMR spectroscopic methods.
    Notes: Es wird über die Darstellung der Mercaptosulfoniumsalze (i-C3H7)2SSX+SbCl6- (X = H, D) und der Chlorthiosulfoniumsalze (i-C3H7)2SSCl+MF6- (M = As, Sb) und (i-C3H7)2SSSCl+SbCl6- berichtet. Sie werden aus chloriertem oder protoniertem (i-C3H7)2S durch Kondensationsraktionen mit überschüssigem H2S oder SCl2 und S2Cl2 gebildet. Die Charakterisierung der Thiosulfoniumverbindungen erfolgt schwingungs- und NMR-spektroskopisch.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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